A kind of preparation method of outer wall fluorinated multi-walled carbon nanotube containing iron fluoride intercalation substance
A technology of multi-walled carbon nanotubes and fluorination, applied in structural parts, electrical components, battery electrodes, etc., can solve problems such as volume expansion and low electronic conductivity, and achieve the effect of increasing output voltage and theoretical specific capacity
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Embodiment 1
[0034] In this embodiment, the preparation method of the outer wall fluorinated multi-walled carbon nanotubes containing iron fluoride intercalation comprises the following steps:
[0035] 1. Mix the dry multi-walled carbon nanotubes with KOH evenly, and react in a tube furnace at 700°C for 4 hours under a nitrogen atmosphere, then cool to room temperature, wash with water, and then dry. After drying, it is mixed with concentrated nitric acid (concentration: 68wt%) of 40 times the mass ratio, refluxed at 80° C. for 2 hours, and then washed with water until neutrally dried.
[0036] 2. Place the high-purity multi-walled carbon nanotubes with the end caps opened in a dry, vacuumable heating reactor, and feed ferric chloride vapor with a mass ratio of 2:1 to the multi-walled carbon nanotubes at 330°C React for 6 hours, so that ferric chloride intercalates into the multi-walled carbon nanotubes. After the reaction, the temperature is lowered to 310° C., and the process pressure is...
Embodiment 2
[0042] In this embodiment, the preparation method of the outer wall fluorinated multi-walled carbon nanotubes containing iron fluoride intercalation comprises the following steps:
[0043] 1. Mix the dried multi-walled carbon nanotubes with NaOH evenly, react in a tube furnace at 750°C for 4 hours under a nitrogen atmosphere, then cool to room temperature, wash with water and then dry. After drying, mix with 30 times mass ratio fuming concentrated nitric acid (concentration 85wt%), reflux at 90°C for 2 hours, then wash with water until neutral drying.
[0044] 2. Place the high-purity multi-walled carbon nanotubes with the end caps opened in a dry, vacuumable heating reactor, and feed ferric chloride vapor with a mass ratio of 2:1 to the multi-walled carbon nanotubes at 320°C React for 6 hours, so that ferric chloride intercalates into the multi-walled carbon nanotubes. After the reaction, the temperature is lowered to 310° C., and the process pressure is maintained at 0.3 MPa...
Embodiment 3
[0049] In this embodiment, the preparation method of the outer wall fluorinated multi-walled carbon nanotubes containing iron fluoride intercalation comprises the following steps:
[0050] 1. Mix the dry multi-walled carbon nanotubes with KOH evenly, react in a tube furnace at 730°C for 5 hours under a nitrogen atmosphere, then cool to room temperature, wash with water and then dry. After drying, it is mixed with concentrated hydrochloric acid (concentration 35wt%) of 80 times the mass ratio, refluxed at 80° C. for 3 hours, and then washed with water until neutrally dried.
[0051] 2. Place the high-purity multi-walled carbon nanotubes with the end caps opened in a dry, vacuumable heating reactor, and feed ferric chloride vapor with a mass ratio of 2:1 to the multi-walled carbon nanotubes at 315°C React for 6 hours, so that ferric chloride intercalates into the multi-walled carbon nanotubes. After the reaction, the temperature is lowered to 310° C., and the process pressure is...
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